Process of treating oils.



No. 769,681. PATENTED SEPT. 6, 1904. A. G. CALKINS.

PROCESS OF TREATING OILS.

APPLIOATION FILED SEPT. 2a, 1902.

no MODEL.

WVz'frzeail QM (I C /M 5 $63. W AM ffZ/Wfl UNITED STATES PatentedSeptember 6, 1904:.

PATENT FFICE.

ALBERT C. CALKINS, OF LOS ANGELES, CALIFORNIA, ASSlG-NOR OF ONE- HALF TOHENRY E. BRETT, OF LOS ANUELES, CALIFORNIA.

PROCESS OF TREATING OILS- SPECIFICATION forming part of Letters PatentNo. 769,681, dated September 6, 1904.

Application filed $eptember 23,1902. Serial No. 124,583. (No specimens.)

To (LZZ who/1t it WMLZ/ concern:

Be it known that LALB ear G. UALKINs, a citizen of the United States,residing at Los Angeles, in the county of Los Angeles and State 5 ofCalifornia, have invented certain new and useful Improvements inProcesses of Treating Oils; and I do hereby declare the following to bea full, clear, and exact description of the invention, such will enableothers skilled in the art to which it appertains to make and use thesame.

This invention relates to improvements in the process or method oftreating and retining of oils and similar fluids, and 1 )art-icularly 5such oils as contain asphaltum and similar impurities and which it isdesired to treat by acid whose oxidizing effect upon the anilincoloringmatter in the oils is beneficial and which acid will alsopercipitate the asphaltum,

so that the treated oil will be suitable in quali ty and color forlubricating stock; and one of the objects of this invention is toproduce a process or method which will avoid the loss of the lighterdistillates during the treatment of the oil.

Another object of the invention is to use the agitating medium more thanonce in a complete circuit and to use the lighter serials in combinationwith a fluid as an agitating me- 0 dium.

'ith these and other objects in view the invention consists,essentially, in the method or process hereinafter more fully described,and substantially as illustrated in the accompanying drawing, showingone form of apparatus that may be employed in carrying out the processor method.

.In the treatment of oil containing asphaltum it is found that evenafter distillation a cer- 4 tain amount of asphaltum will remain in theoil, and the treating process must be resorted to to eliminate whatremains. Ordinarily the excess of residual acid is neutralized by theuse of some alkali, such as caustic soda, and

these successive operations are all performed in a tank havinga conicalbottom and suitable connections for drawing 03' the precipitated acidcompounds, &C. The mixing of the acid with the oil is performed by meansof a blow- 5 ing-engine arranged to deliver air or other agitatingmedium through a pipe leading down into the tank or receptacle, so thatthe violently-rising air creates active ebullition in the tank andexposes all of the oil to the action of the acid. In fact, the action ofthe air practically atomizes the oil and acid and makes as perfect amixture and exposure to the acid as can be obtained by mechanical means.lVhen this operation is performed in a tank or receptacle open at itstop, a large percentage of the lighter fractionsin the oil isnecessarily evaporated and driven off with the air, which is beingconstantly forced up through the oil, and this loss is serious in thetreatment of oil containing light distillatcs which are 5 used for theirexplosive nature in gasolene and vapor engines, as these lighter serialsthat are so readily evaporated and carried off by the.

. air frequently constitute the most valuable part of the distillate forengine use. 7

By means of this invention the loss of the lighter distillates isavoided by treating the oil in a closed treating tank or receptacle andwithdrawing the air or agitating medium forced in by the blowing-engineto again supply such engine, so that there will be a com pletecirculation or circuit of the air or agitating medium through the tank.

Referring now to the drawing forming part of this application, there isshown one 30 form of apparatus which may be employed in carrying out theherein-described process or method, although this invention is in nomanner limited to use with such apparatus.

Upon the drawing the reference character 5 1 designates a tank or othertreatingrecepta cle, preferably provided with a top or cover 2,completely closing the tank, in which there may be formed a manhole 3 toafford access to the interior of the tank or receptacle, which 9 lattermay be supported upon any suitable structure by means of brackets 4, andthe tank 1 may be provided with a suitable valved outlet 5 for thepurpose of withdrawing any asphaltum or tarry compound, and the tank orreceptacle is preferably unobstructed interiorly by any cross-plates,partitions, or other barriers. A suitable pipe or connection 6 may beprovided, preferably at the top of the tank, through which the oil maybe introduced thereinto, and a connection 7 may be provided between thetop of the tank and any suitable form of blowing-engine 8 or equivalentdevice to supply air to the blowing-em gine, and a discharge-pipe 9 ispreferably secured in and depends from the top of the tank to nearly thebottom thereof in order to liberate the air or agitating medium at ornear the bottom of the tank or receptacle, so that the same can risetherethrough and agitate the contents thereof, as Will be readilyunderstood.

Connected with the exposed end of the discharge-pipe 9 is a suitablepipe 10, communicating with the blowing-engine 8, so that the air oragitating medium is forced by the engine 8 through the pipe orconnection 10 into and through the discharge-pipe 9, from which the airor agitating medium is liberated to rise, substantially as hereinbeforeexplained.

The pipe or connection 7 is preferably provided with a suitable cut-offor valve 11 for the purpose of closing the suction-pipe or connection 7whenever it is desired to use the same in the manner now in vogue, whichmay be done by removing the cover of the manhole 3 and turning saidcut-off or valve 11 so as to admit air therethrough to the engine 8,whereupon the engine will take air in the ordinary manner, and the airwill escape through the manhole after having passed through the contentsof thetank or receptacle.

It is found that after an asphalt-base oil has been run or distilled forthe asphaltum contained the distillate or the product from which theasphaltum has been eliminated by distillation still contains from ten totwenty per cent. of tarry matter that can only be removed by acidtreatment, and the tarry compound which is precipitated out of thedistillate by a sulfuric-acid treatment is of a consistency of heavycoal-tar, and as the precipitations of the tar commences the moment theacid comes in contact with the oil it is only necessary for the tankl'to be entirely unobstructed interiorly, as otherwise it wouldimmediately clog and it would be impossible to remove the tar.

1n the use of the construction herein shown and described theprecipitated compounds settle into the conical bottom of the tank 1 andare drained off through the large outlet pipe or connection 5, which isdesirably provided with a cook or cut-off 12 of any suitableconstruction. The consistency, thickness, and volume of the tarrymaterial which is removed by the acid treatment is such that in thetreatment of heavy asphaltic oils the outletpipe 5 is preferably made oflarge diameter to facilitate the withdrawal of this material.

By the use of the closed unobstructed tank described and shown hereinshould the oil being treated be too heavy and viscous to permit airagitation a volatile oil may be added to thin the heavy oil and none ofthe added volatile oil will be lost. during the agitation.

None of the vapor taken up by the air is removed or condensed by theapparatus herein shown and described, and no fresh air is admittedduring the treating operation; but the treatment is effected without anyloss of distillates and without the admission of any atmospheric airafter the operation has commenced, and in case too much pressure shouldaccumulate in the tank by the rapid generation of sulfurous-acid gas thetank may be vented through the valved pipe or connection 6, which mayalso be employed for supplying oil to the tank; but oil may also beintroduced through the manhole 3, if found desirable in practice.

The operation of this invent-ion in connection with the apparatusillustrated in the accompanying drawing is substantially as follows, towit: First a suitable amount of oil is introduced within the treatingtank or receptacle, and the desired quantity of sulfuric acid is addedor supplied, whereupon the sulfuric acid will be broken up or bedecomposed when it comes in contact with and attacks the oil containingthe carbon compounds in solution. and when the acid decomposes a largepercentage of sulfurous-acid gas is generated, but is prevented fromescaping into the outer air by reason of the tank or receptacle beingclosed. This sulfurous-acid gas is withdrawn through the suction-pipe 7by the action of the blowing-engine 8 and is forced back to the treatingtank or receptacle through the connection 10 into and through thedischargepipe 9 and liberated at the bottom of the treating tank orreceptacle in such a manner as to cause this gas to rise up through andagitate the contents of the tank, as will bev readily understood.

By means of this process or method of treat ing oil the sulfurous-acidgas is passed and repassed through the oil, whereby a double effect isattained of precipitating the tar and acid compounds thereof, as Well ashaving the benefit of the bleaching effect of the sulfurousacid gas,which is known to be one of the best, if not the greatest, of bleachingagents, and by means of this invention it is possible to so pass andrepass the sulfurous-acid gas through the tank without any materialchange in the gas, as all condensing agents between the tank and theblower are avoided.

By means of this process or method there is secured a return of thegenerated sulfurousacid gas in bleaching-and treating the oil for color,and this gas will be generated in the treatment of the oil by the acidfor precipitating the tarry matter in the oil, substantially as beforedescribed.

From the foregoing it will appear that in the apparatus herein shown anddescribed there is an interiorlyunobstructed treating tank or receptacleto prevent clogging by the precipitated tarry matter, a closed treatingtank or receptacle to avoid the loss of any light distillates and toprovide means whereby air or an agitating medium may be forced 3 againand again through the oil or material to be treated in a continuouscircuit and the j sulfurous-acid-gas fumes be returned through andthrough the mass of oil without subjecting the user to the loss of thelight distillates.

From the foregoing description and the accompanying drawing it will beunderstood that this method or process of treating oil or othermaterials consists substantially in sub jecting the oil to the action ofacid within a closed interiOrly-unobstructed treating tank or receptacleto produce a precipitation of the tarry matter in the oil, then toproduce an upward circulation of air from the bottom to the top of saidtank by means of a blower. whose suction-pipe is connected with the topof the tank while its discharge-pipe discharges to the lower portion ofthe tank, the suction and discharge pipes being free of condensers, sothat the oil may be acid-treated and may be subjected to the blowingaction for producing ebullition without the loss of the lighterdistillates and the sulfurous acid gas generated within the tank may bereturned through the same means used in producing the ebullition withoutany resulting condensation of the gas.

It is not desired to confine this invention to the specific apparatusherein shown and described for carrying out this process or method, asit will be understood that any suitable apparatus may be employed forthis purpose without departing from the spirit and scope of thisinvention.

1 claim- 1. The herein-described process or method of treating oil orother fluids which consists in confining the oil within a closedtreating receptacle or tank; subjecting the oil to the action ofsulfuric acid to precipitate tarry matters within the oil withdrawingthe sulfurousacid gas generated within the tank and return- I ing thesame to and through the contents of l the tank to bleach and agitate theoil.

2. The herein-described process or method of treating oil or otherfluids which consists in subjecting the oil to the action of an acidwhile in a closed treating receptacle or tank introducing an agitatingmedium through. the oil; withdrawing the lighter vapors from above theoil and returning the same together with the agitating medium andevolved gas to and through the oil and acid to facilitate the treatmentof the oil.

3. The herein-described process or method of treating oil or otherfluids which consists in subjecting the oil to the action of an acid;then introducing an agitating medium through the oil and returning toand through the oil and acid in a continuous circuit the agitatingmedium and fluids generated by the action of the acid to agitate theacid and oil.

4:. The herein-described process or method of treating oil or otherfluids which consists in subjecting the oil to the action of sulfuricacid while in a closed treating receptacle or tank; withdrawing the airand the evolved gas from above the oil and passing and repassing thesame continuously up through the oil and acid to agitate the oil andacid and to subject the oil to the bleaching action of the evolved gas.

5. The herein-described process or method of treating oil or otherfluids which consists in confining the oil within a closed receptacle;subjecting the oil while in such receptacle to the action of sulfuricacid to precipitate the tarry matters in the oil; withdrawing the airabove the oil and liberating the same below the oil to rise therethroughand agitate the same and finally passing and repassing the con1- mingledair and sulfurous-acid gas evolved by the action of the acid on the oilto bleach the oil by the action of said gas.

In testimony whereof l have signed my name to this specification, in thepresence of two subscribing witnesses, at Los Angeles, in the county ofLes Angcles and State of California, this 12th day of September, 1902.

ALBERT (J. GALKINS.

\Vitnesses:

AMELIA UrUusT, R. E. BRINKER.

